CN105133319B - Preparation method of molten-drop-resisting polyamide fiber or fabric - Google Patents
Preparation method of molten-drop-resisting polyamide fiber or fabric Download PDFInfo
- Publication number
- CN105133319B CN105133319B CN201510613344.4A CN201510613344A CN105133319B CN 105133319 B CN105133319 B CN 105133319B CN 201510613344 A CN201510613344 A CN 201510613344A CN 105133319 B CN105133319 B CN 105133319B
- Authority
- CN
- China
- Prior art keywords
- fabric
- fiber
- preparation
- dropping
- fypro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000004744 fabric Substances 0.000 title claims abstract description 110
- 239000000835 fiber Substances 0.000 title claims abstract description 79
- 239000004952 Polyamide Substances 0.000 title claims abstract description 26
- 229920002647 polyamide Polymers 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000000178 monomer Substances 0.000 claims abstract description 26
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 10
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- 238000010894 electron beam technology Methods 0.000 claims description 29
- 238000009835 boiling Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 7
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 claims description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 7
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 7
- 238000004132 cross linking Methods 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 5
- 150000001261 hydroxy acids Chemical group 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 4
- 239000011976 maleic acid Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 3
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 239000004753 textile Substances 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000008093 supporting effect Effects 0.000 abstract description 4
- 230000006378 damage Effects 0.000 abstract description 3
- 229920001519 homopolymer Polymers 0.000 abstract description 3
- 230000005855 radiation Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 239000003610 charcoal Substances 0.000 description 15
- 238000002485 combustion reaction Methods 0.000 description 15
- 230000001965 increasing effect Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 8
- 239000003063 flame retardant Substances 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000011260 aqueous acid Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 229920000578 graft copolymer Polymers 0.000 description 3
- 239000012209 synthetic fiber Substances 0.000 description 3
- 229920002994 synthetic fiber Polymers 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 description 1
- 206010072170 Skin wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- -1 additionally Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000001976 improved effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 201000007094 prostatitis Diseases 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a preparation method of molten-drop-resisting polyamide fiber or fabric. Under a normal temperature air condition, the fiber or fabric is radiated by virtue of electronic beams, then the fiber or fabric is placed into a monomer aqueous solution containing carboxyl groups to be under pre-reaction, and the fiber or fabric is enabled to be self-cross linked; then the fiber or fabric is padded in a polymerization inhibitor and a compound aqueous solution consisting of two monomers containing reactive double bonds, and the electronic beam radiation grafting is carried out after twice impregnation and twice rolling; after the grafting reaction is completed, the fiber or fabric can be boiled by virtue of treatment liquid so as to remove a grafted homopolymer to obtain the molten-drop-resisting polyamide fiber or fabric. The preparation method is simple and easy to operate and capable of implementing the industrialized production, and during a burning process of the prepared molten-drop-resisting polyamide fiber or fabric, a carbonized supporting layer can be rapidly formed on the surface of the fiber or fabric, so that the formation of molten drops is effectively inhibited, and the secondary harm caused by a high-temperature flame dropping object is avoided, and the situation threatening the human life can be prevented.
Description
Technical field
The present invention relates to the preparation method of a kind of fiber or fabric, more particularly, to a kind of anti-dropping Fypro
Or the preparation method of fabric.
Background technology
Fypro is a kind of relatively early synthetic fibers for realizing industrialized production, and its yield occupies always each synthetic fibers
Prostatitis, because its have the performances such as good elasticity, strength, rub resistance weaving etc. relevant industries have a wide range of applications.
With the higher pursuit of the development and people of social production to quality of the life, to traditional weaving synthetic fibers material
Material proposes harsher requirement, such as requires that it has certain fire resistance under many occasions.Fatty polyamide is fine
Dimension belongs to combustible, and the value of its limited oxygen index is about 20～21.5, with serious drip phenomenon during burning.These high temperature drops
Junk easily ignites other materials, accelerates flame propagation, expands fire scale；If drop in that serious scalding can be caused on human body skin
Wound is even burnt, and brings secondary injury, be significantly limit it and is built in underwear, protective garment, military training clothes and some high levels
The application built.
For the inflammable problem of fiber, carried out altogether by adding fire retardant during fiber synthesis phase or melt spinning
Poly- or co-blended spinning and flame-retardant after-finishing is carried out to fabric, can substantially realize the fire-retardant of fiber.But for molten drop problem does not have
There is effective solution, and the fire-retardant mechanism of many products is all built upon on the basis of molten drop on market, it is intended to pass through
Reducing fusing point, reinforcement melting drippage departs from Combustion Source to reach fire-retardant purpose, therefore solves in fibrous material combustion process
Molten drop problem seem particularly urgent.
Prepare the Fypro with anti-dropping effect or fabric it is critical only that the flowing for reducing melt in combustion process
Property, the intensity of melt is improved, through the joint efforts of Chinese scholars, at present can be by physics increasing stick, into charcoal effect, in fibre
Dimension table face forms the mechanism such as supporting layer and change material structure to reach the purpose of anti-dropping.Such as add polytetrafluoroethyl-ne in fiber
Alkene powder, clay, talcum powder etc. reduce the mobility of melt, although the method can reduce molten drop increasing the viscosity of melt
Number, but for the flammability of molten drop is without improvement；Managed using the condensed phase charcoal forming machine of some fire retardants, promoted in combustion
Enter matrix into charcoal, improve the anti-dropping performance of material, but there is fire-retardant FRW complex process, the high problem of development cost.
The content of the invention
It is an object of the invention to provide the preparation method of a kind of anti-dropping Fypro or fabric, the method has place
Reason is uniform, efficiency high, pollution less, technological process it is simple and the features such as be easily achieved industrialization, prepared fiber or fabric is anti-
Melt-dropping property is excellent, stable and durable effect, and washability is good.
The present invention is as follows using technical scheme：
(1) under the conditions of normal temperature air, synthetic polyamide fiber or fabric are carried out into electron beam irradiation, is put immediately after irradiation
Enter in the monomer solution containing hydroxy-acid group carries out pre-reaction at 60～80 DEG C of constant temperature, makes selfing between polyamide molecule
Connection；
(2) by the fiber or textile pad after pre-reaction in polymerization inhibitor and by two kinds of monomer compositions containing reactive double bond
Compound water solution in, the liquid carrying rate that the fiber or fabric are caused after two leachings two are rolled is 60～100%, then carries out electricity
Beamlet irradiation grafting；
Polymerization inhibitor adopts Fe2SO4, the mass percentage concentration of polymerization inhibitor is 0.05～0.15%；Two kinds contain reactive double bond
Monomer be respectively one kind and hydroxyethyl methacrylate and acrylic acid hydroxyl in acrylamide and N hydroxymethyl acrylamide
One kind in propyl ester, the mass percentage concentration ratio respectively 10～20% between two kinds of monomers：5～10%；
(3) after the completion of graft reaction, boiling is carried out to fiber obtained above or fabric with treatment fluid and is boiled, it is equal to remove grafting
Polymers, that is, obtain described anti-dripping fibre or fabric.
Thermostat temperature preferably can be 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C or 80 DEG C in the step (1).
The irradiation dose of electron beam irradiation is 80～120kGy in the step (1).Preferably can be 80kGy, 100kGy
Or 120kGy.
The preferred concentration of the polymerization inhibitor can be 0.05%, 0.10% or 0.15%.
The preferred concentration of described two monomers can be respectively 10%:5%th, 10%:10%th, 15%:5%th, 15%:10%th,
20%:5% or 20%:10%.
In the step (1), the monomer containing hydroxy-acid group is acrylic acid, methacrylic acid, maleic acid or clothing health
One kind in acid, the mass percentage concentration of monomer solution is 10%.
The pre-reaction of the step (1) is carried out in thermostat water bath, and reaction temperature is 60～80 DEG C.
The step (2) two soak two roll process in, the pressure between double roller be 0.1～0.3Mpa, concretely 0.1MPa,
0.2MPa or 0.3MPa, rotating speed is 6m/min.
The irradiation dose of step (2) the electron beam irradiation graft reaction be 90～180kGy, preferably can for 90kGy,
135kGy or 180kGy.
Described treatment fluid is a kind of aqueous solution in NaOH, sodium carbonate, sodium acid carbonate, sodium phosphate, ammonium hydrogen carbonate, is located
The mass percentage concentration of reason liquid is 1～4%, preferably can be 1%, 2% or 4%.
The fiber or fabric are the fiber or fabric of synthesizing polyamides.
The fabric can be the uni-material fabric or blend fabric of above-mentioned Fypro, concretely woven fabric, knitted fabric
And non-woven fabrics.
What the technical method adopted in the present invention realized that the anti-dropping of Fypro or fabric utilizes is following principle：
The class monomer containing hydroxy-acid group can promote the crosslinking between polyamide molecule under certain reaction condition, and cross-linked structure can
Realize not melting for material；In graft reaction between monomer and polyamide macromolecular formed graft polymers, when being heated prior to
Matrix decomposes and forms coke layer and provides support for fiber melt, additionally, it also has the effect for promoting matrix into charcoal, by matrix
The melting behavior of material is converted into into charcoal process, and meeting accompanying drawing is specifically described in embodiment of these principles below.
Mainly irradiation crosslinking technological is applied in terms of anti-dropping in existing radiation processing technology, by adding in material
Plus it is aided with irradiation after crosslinking agent, and make material internal produce crosslinking, thermosetting is changed into by thermoplasticity, so as to realize not melting, but mesh
It is front mainly still to concentrate on plastic industry.The present invention causes some to have into the monomer of charcoal effect using the inductive effect of electron beam
Carry out graft reaction, promote matrix material into charcoal, the melting behavior of matrix is converted into into into charcoal process.With irradiation processing skill
The gradually maturation of art, application of the present invention in terms of fabric modifying has very big potentiality.
Compared to existing technology method generates following different know-why to the present invention, has the advantages that：
The effect of anti-dropping is heavily dependent on the removal efficiency of the grafting efficiency of monomer and grafting accessory substance, meaning
Will improve monomer concentration, and concentration certainly will cause the autohemagglutination between monomer to aggravate while increase, be unfavorable for being grafted accessory substance
Remove, the method used in the present invention has efficiently controlled the generation of monomer homopolymers, farthest improves connecing for monomer
Branch efficiency, is mainly reflected in three below aspect：
A) present invention carries out cross-linking radiation using the method for pre-irradiation to fiber or fabric, and monomer is not received in the inventive method
The irradiation of electron beam, the probability that autohemagglutination occurs between monomer is low, because the reaction is relatively mild, can avoid the mistake between polyamide molecule
Degree is crosslinked and the performance of impact material；
B) present invention is firstly introduced polymerization inhibitor in grafting system, and by continuous experimental exploring the inhibition of the concentration is obtained
Agent can effectively suppress the autohemagglutination between monomer, improve the grafting efficiency of graft reaction；
C) carry out boiling to the fiber or fabric obtained by reaction with treatment fluid to boil, removal efficiency of the method to monomer homopolymers
Height, the fiber or fabric for having processed has good feel.
The preparation method being related in the present invention is carried out after spinning, does not change the original production technology of fiber, and
Less is destroyed to fiber molecule agent structure, cross-linking effect more preferably, farthest retains the original performance of fiber or fabric, such as
Intensity, feel etc.；Monomer is introduced in the side chain of fiber molecule by covalently bound mode and ensure that modified persistence.
The preparation method that the present invention is provided is simple, it is easy to accomplish industrialization production, the anti-dripping fibre of preparation or knits
In combustion surface energy quickly forms charing supporting layer to thing, not molten drop, the harm that high temperature molten drop thing can be avoided to bring, resistance
The situation for only jeopardizing people's life occurs.
Description of the drawings
Fig. 1 is the thermogravimetric curve figure of polyamide anti-dropping fabric prepared by the present invention.
Fig. 2 is the surface topography of residue after polyamide anti-dropping fabric prepared by the present invention and its calcination.
Specific embodiment
With reference to the accompanying drawings and examples the invention will be further described.
Experimental technique used in following embodiments if no special instructions, is conventional method.
Material used, reagent etc. in following embodiments, such as without Special Statement, commercially obtain.
Percentage composition described in following embodiments is weight/mass percentage composition.
Embodiments of the invention are as follows：
Embodiment 1：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to Fypro, make dosage reach 80kGy, after irradiation
Fiber be immediately placed in 10% acrylic acid aqueous solution, and 1h is reacted at 60 DEG C, wash clean after reaction, fiber is without substantially increasing
Weight, then pads Fypro by 10% acrylamide and 5% hydroxyethyl methacrylate and 0.05%
Fe2SO4Mixed aqueous solution in a period of time, allow fiber by padding machine, the pressure between double roller is 0.3Mpa, makes fiber liquid carrying rate
60% is reached, electron beam irradiation grafting is then carried out, makes irradiation dose reach 135kGy, after irradiation grafting, use 1% NaOH
Solution boils 20min to fiber boiling, washes clean afterwards, and percent grafting is 11.4%.
In combustion, surface carbonizes rapidly the present embodiment gained fiber, does not drip, and illustrates that the fiber for preparing has anti-
The characteristic of molten drop.
Embodiment 2：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to Fypro, make dosage reach 120kGy, after irradiation
Fiber be immediately placed in 10% metering system aqueous acid, and 1h is reacted at 70 DEG C, wash clean after reaction, fiber is without bright
Aobvious weightening, then pads Fypro by 12% acrylamide and 8% hydroxypropyl acrylate and 0.05%
Fe2SO4Mixed aqueous solution in a period of time, allow fiber by padding machine, the pressure between double roller is 0.2Mpa, makes fiber liquid carrying rate
80% is reached, electron beam irradiation grafting is then carried out, makes irradiation dose reach 180kGy, it is molten with 2% sodium carbonate after irradiation grafting
Liquid boils 20min to fiber boiling, washes clean afterwards, and percent grafting is 15.6%.
In combustion, surface carbonizes rapidly the present embodiment gained fiber, does not drip, and illustrates that the fiber for preparing has anti-
The characteristic of molten drop.
Embodiment 3：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to Fypro, make dosage reach 100kGy, after irradiation
Fiber be immediately placed in the 10% itaconic acid aqueous solution, and 1h is reacted at 65 DEG C, wash clean after reaction, fiber is without substantially increasing
Weight, then Fypro is padded by 20% N hydroxymethyl acrylamide and 5% hydroxypropyl acrylate and
0.10% Fe2SO4Mixed aqueous solution in a period of time, allow fiber by padding machine, the pressure between double roller is 0.3Mpa, makes fibre
Dimension liquid carrying rate reaches 60%, then carries out electron beam irradiation grafting, makes irradiation dose reach 90kGy, after irradiation grafting, uses 4%
Sodium bicarbonate solution boils 20min to fiber boiling, washes clean afterwards, and percent grafting is 13.4%.
In combustion, surface carbonizes rapidly the present embodiment gained fiber, does not drip, and illustrates that the fiber for preparing has anti-
The characteristic of molten drop.
Embodiment 4：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to Fypro, make dosage reach 120kGy, after irradiation
Fiber be immediately placed in 10% metering system aqueous acid, and 1h is reacted at 80 DEG C, wash clean after reaction, fiber is without bright
Aobvious weightening, then Fypro is padded by 20% N hydroxymethyl acrylamide and 10% hydroxypropyl acrylate and
0.15% Fe2SO4Mixed aqueous solution in a period of time, allow fiber by padding machine, the pressure between double roller is 0.1Mpa, makes fibre
Dimension liquid carrying rate reaches 100%, then carries out electron beam irradiation grafting, makes irradiation dose reach 180kGy, after irradiation grafting, uses
2% sodium radio-phosphate,P-32 solution boils 20min to fiber boiling, washes clean afterwards, and percent grafting is 19.1%.
In combustion, surface carbonizes rapidly the present embodiment gained fiber, does not drip, and illustrates that the fiber for preparing has anti-
The characteristic of molten drop.
Embodiment 5：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to Fypro, make dosage reach 80kGy, after irradiation
Fiber be immediately placed in 10% aqueous maleic acid, and 1h is reacted at 75 DEG C, wash clean after reaction, fiber is without substantially increasing
Weight, then pads Fypro by 10% acrylamide and 10% hydroxyethyl methacrylate and 0.05%
Fe2SO4Mixed aqueous solution in a period of time, allow fiber by padding machine, the pressure between double roller is 0.1Mpa, makes fiber liquid carrying rate
80% is reached, electron beam irradiation grafting is then carried out, makes irradiation dose reach 135kGy, after irradiation grafting, use 1% ammonium hydrogen carbonate
Solution boils 20min to fiber boiling, washes clean afterwards, and percent grafting is 14.6%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fiber for preparing has anti-
The characteristic of molten drop.
Embodiment 6：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to polyamide fabric, make dosage reach 120kGy, after irradiation
Fabric be immediately placed in 10% metering system aqueous acid, and 1h is reacted at 80 DEG C, wash clean after reaction, fabric is without bright
Aobvious weightening, polyamide fabric is then padded the hydroxyethyl methacrylate in the N hydroxymethyl acrylamide by 20% and 5%
And 0.10% Fe2SO4Mixed aqueous solution in a period of time, allow fabric by padding machine, the pressure between double roller is 0.3Mpa,
Make fabric liquid carrying rate reach 60%, then carry out electron beam irradiation grafting, make irradiation dose reach 135kGy, after irradiation grafting,
20min is boiled to fabric boiling with 4% ammonium bicarbonate soln, washes clean afterwards, percent grafting is 16.7%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric for preparing has anti-
The characteristic of molten drop.
Embodiment 7：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to polyamide fabric, make dosage reach 120kGy, after irradiation
Fabric be immediately placed in the 10% itaconic acid aqueous solution, and 1h is reacted at 60 DEG C, wash clean after reaction, fabric is without substantially increasing
Weight, then pads polyamide fabric by 14% acrylamide and 6% hydroxyethyl methacrylate and 0.10%
Fe2SO4Mixed aqueous solution in a period of time, allow fabric by padding machine, the pressure between double roller is 0.2Mpa, makes fabric liquid carrying rate
80% is reached, electron beam irradiation grafting is then carried out, makes irradiation dose reach 135kGy, after irradiation grafting, use 4% sodium acid carbonate
Solution boils 20min to fabric boiling, washes clean afterwards, and percent grafting is 16.3%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric for preparing has anti-
The characteristic of molten drop.
Embodiment 8：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to polyamide fabric, make dosage reach 80kGy, after irradiation
Fabric be immediately placed in 10% acrylic acid aqueous solution, and 1h is reacted at 65 DEG C, wash clean after reaction, fabric is without substantially increasing
Weight, then polyamide fabric is padded by 20% N hydroxymethyl acrylamide and 10% hydroxypropyl acrylate and
0.15% Fe2SO4Mixed aqueous solution in a period of time, allow fabric by padding machine, the pressure between double roller is 0.1Mpa, makes to knit
Thing liquid carrying rate reaches 100%, then carries out electron beam irradiation grafting, makes irradiation dose reach 180kGy, after irradiation grafting, uses
2% sodium radio-phosphate,P-32 solution boils 20min to fabric boiling, washes clean afterwards, and percent grafting is 19.7%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric for preparing has anti-
The characteristic of molten drop.
Embodiment 9：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to polyamide fabric, make dosage reach 100kGy, after irradiation
Fabric be immediately placed in 10% aqueous maleic acid, and 1h is reacted at 75 DEG C, wash clean after reaction, fabric is without substantially increasing
Weight, then pads polyamide fabric by 10% acrylamide and 5% hydroxypropyl acrylate and 0.05% Fe2SO4
Mixed aqueous solution in a period of time, allow fabric by padding machine, the pressure between double roller is 0.1Mpa, reaches fabric liquid carrying rate
100%, electron beam irradiation grafting is then carried out, make irradiation dose reach 180kGy, it is molten with 1% NaOH after irradiation grafting
Liquid boils 20min to fabric boiling, washes clean afterwards, and percent grafting is 13.3%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric for preparing has anti-
The characteristic of molten drop.
Embodiment 10：
Under the conditions of normal temperature air, first electron beam irradiation is carried out to polyamide fabric, make dosage reach 80kGy, after irradiation
Fabric be immediately placed in 10% acrylic acid aqueous solution, and 1h is reacted at 70 DEG C, wash clean after reaction, fabric is without substantially increasing
Weight, then polyamide fabric is padded by 10% N hydroxymethyl acrylamide and 10% hydroxyethyl methacrylate and
0.05% Fe2SO4Mixed aqueous solution in a period of time, allow fabric by padding machine, the pressure between double roller is 0.3Mpa, makes to knit
Thing liquid carrying rate reaches 60%, then carries out electron beam irradiation grafting, makes irradiation dose reach 90kGy, after irradiation grafting, uses 2%
Sodium carbonate liquor boils 20min to fabric boiling, washes clean afterwards, and percent grafting is 11.2%.
In combustion, surface carbonizes rapidly the present embodiment gained fabric, does not drip, and illustrates that the fabric for preparing has anti-
The characteristic of molten drop.
The thermogravimetric curve of anti-dropping fabric sample prepared in above-described embodiment 8 is as shown in figure 1, wherein square is represented
As former state, triangle represents the fabric sample prepared in the present embodiment to polyamide fabric；It is fine in prepared anti-dropping fabric sample
The surface topography of dimension and its in high temperature Muffle furnace after calcination 20 minutes the surface topography of gained residue as shown in Fig. 2 wherein
A it is as former state, (b) fabric sample prepared in the present embodiment with (d) that () and (c) is fabric.
The temperature of initial decomposition of fabric former state is can be seen that at 372 DEG C, this enforcement from the thermogravimetric curve of Fig. 1 fabric samples
Fabric sample temperature of initial decomposition is advanced to 173 DEG C in example, and mainly graft polymers decomposes in advance what is caused, glycerol polymerization
The introducing of thing promotes the decomposition of matrix, additionally, charcoal residual rate of the sample at 800 DEG C is increased to by the 3.5% of fabric former state
8.6%, 1.5 times are increased, show the fabric sample for using the preparation method in this patent to prepare, its carbon-forming performance is substantially carried
Rise, the most melting behavior of matrix can be converted into harmless into charcoal process.
Fiber in the anti-dropping fabric that will be prepared in embodiment 8 observes under a scanning electron microscope surface topography, from
As can be seen that, its fiber surface is smooth and flat for fabric as former state in Fig. 2 (a), arrange loose between fiber, it is interfibrous
Space is high-visible.And in the sample after grafting, such as shown in Fig. 2 (b), fiber surface becomes coarse and covers to have gone up one layer
Graft polymers, the trend for having entanglement between fiber is more tight when arranging situation is also more non-grafted.Can be with from Fig. 2 (c)
Find out the layer of charcoal surface relatively flat of fabric former state, the loose intensity of layer of charcoal is not high.For grafting samples, shown in such as Fig. 2 (d), charcoal
Layer surface presents similar cellular cross-linked structure, illustrates to there occurs crosslinking inside the fabric sample in the present embodiment, and charcoal
Layer is more abundant, and closely cross-linked structure can improve the intensity of layer of charcoal, be that fiber melt is provided a supporting role, and suppress its melting drop
Fall, more than reflect that the present invention has the significant technique effect of protrusion.
The specific embodiment of above-mentioned specific embodiment is used for illustrating the present invention, rather than limits the invention,
In the protection domain of spirit and claims of the present invention, any modifications and changes made to the present invention both fall within this
Bright protection domain.
Claims (9)
1. the preparation method of a kind of anti-dropping Fypro or fabric, comprises the steps：
(1) under the conditions of normal temperature air, synthetic polyamide fiber or fabric are carried out into electron beam irradiation, is immediately placed in after irradiation and contains
Have in the monomer solution of hydroxy-acid group carries out pre-reaction at 60～80 DEG C of constant temperature, makes self-crosslinking between polyamide molecule；
(2) by the fiber or textile pad after pre-reaction add have polymerization inhibitor by two kinds of monomer groups containing reactive double bond
Into compound water solution in, the liquid carrying rate that the fiber or fabric are caused after two leachings two are rolled is 60～100%, then is carried out
Electron beam irradiation is grafted；
Polymerization inhibitor adopts Fe2SO4, the mass percentage concentration of polymerization inhibitor is 0.05～0.15%；Two kinds of lists containing reactive double bond
Body is respectively the one kind in acrylamide and N hydroxymethyl acrylamide and hydroxyethyl methacrylate and hydroxypropyl acrylate
In one kind, the mass percentage concentration ratio respectively 10～20% between two kinds of monomers：5～10%；
(3) after the completion of graft reaction, boiling is carried out to fiber obtained above or fabric with treatment fluid and is boiled, to remove grafting homopolymerization
Thing, that is, obtain described anti-dripping fibre or fabric.
2. the preparation method of a kind of anti-dropping Fypro according to claim 1 or fabric, it is characterised in that：It is described
The irradiation dose of electron beam irradiation is 80～120kGy in step (1).
3. the preparation method of a kind of anti-dropping Fypro according to claim 1 or fabric, it is characterised in that：It is described
In step (1), the monomer containing hydroxy-acid group is the one kind in acrylic acid, methacrylic acid, maleic acid or itaconic acid, single
The mass percentage concentration of the body aqueous solution is 10%.
4. the preparation method of a kind of anti-dropping Fypro according to claim 1 or fabric, it is characterised in that：It is described
The pre-reaction of step (1) is carried out in thermostat water bath, and reaction temperature is 60～80 DEG C.
5. the preparation method of a kind of anti-dropping Fypro according to claim 1 or fabric, it is characterised in that：It is described
Step (2) two is soaked in two roll process, and the pressure between double roller is 0.1～0.3Mpa, and rotating speed is 6m/min.
6. the preparation method of a kind of anti-dropping Fypro according to claim 1 or fabric, it is characterised in that：It is described
The irradiation dose of step (2) electron beam irradiation graft reaction is 90～180kGy.
7. the preparation method of a kind of anti-dropping Fypro according to claim 1 or fabric, it is characterised in that：It is described
Treatment fluid be NaOH, sodium carbonate, sodium acid carbonate, sodium phosphate, ammonium hydrogen carbonate in a kind of aqueous solution, the quality hundred for the treatment of fluid
Concentration is divided to be 1～4%.
8. the preparation method of a kind of anti-dropping Fypro according to claim 1 or fabric, it is characterised in that：It is described
Fabric is the uni-material fabric or blend fabric of Fypro.
9. the anti-dripping fibre for being prepared according to arbitrary methods described in claim 1-8 or fabric.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510613344.4A CN105133319B (en) | 2015-09-23 | 2015-09-23 | Preparation method of molten-drop-resisting polyamide fiber or fabric |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510613344.4A CN105133319B (en) | 2015-09-23 | 2015-09-23 | Preparation method of molten-drop-resisting polyamide fiber or fabric |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105133319A CN105133319A (en) | 2015-12-09 |
| CN105133319B true CN105133319B (en) | 2017-05-10 |
Family
ID=54718870
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510613344.4A Expired - Fee Related CN105133319B (en) | 2015-09-23 | 2015-09-23 | Preparation method of molten-drop-resisting polyamide fiber or fabric |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105133319B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107177979A (en) * | 2017-06-30 | 2017-09-19 | 四川东材科技集团股份有限公司 | One kind is without molten drop flame retardant polyester fiber/fabric and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102465449A (en) * | 2010-11-10 | 2012-05-23 | 钦焕宇 | Preparation method for pretreated nylon staple fiber |
| CN103173997A (en) * | 2013-03-25 | 2013-06-26 | 中国人民解放军总后勤部军需装备研究所 | Flame-retardant and anti-fusion fiber or fabric and preparation method thereof |
| CN103361978A (en) * | 2012-04-02 | 2013-10-23 | 中国人民解放军总后勤部军需装备研究所 | Method for preparing anti-melting polyester fiber or fabric |
-
2015
- 2015-09-23 CN CN201510613344.4A patent/CN105133319B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102465449A (en) * | 2010-11-10 | 2012-05-23 | 钦焕宇 | Preparation method for pretreated nylon staple fiber |
| CN103361978A (en) * | 2012-04-02 | 2013-10-23 | 中国人民解放军总后勤部军需装备研究所 | Method for preparing anti-melting polyester fiber or fabric |
| CN103173997A (en) * | 2013-03-25 | 2013-06-26 | 中国人民解放军总后勤部军需装备研究所 | Flame-retardant and anti-fusion fiber or fabric and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 改性聚酰胺纤维的开发现状及发展趋势;周卫东;《合成纤维工业》;20141231;第37卷(第1期);第60-65页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105133319A (en) | 2015-12-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101353863B (en) | Method for preparing flame-retardant anti-dripping fibre or fabric and flame-retardant anti-dripping fibre or fabric | |
| CN103173997B (en) | Flame-retardant and anti-fusion fiber or fabric and preparation method thereof | |
| CN102011308B (en) | Environmentally-friendly and long-lasting fire-retarding treatment method for all-cotton knitted fabrics | |
| Lam et al. | Effect of titanium dioxide on the flame‐retardant finishing of cotton fabric | |
| CN107201654A (en) | A kind of washable fire-retardant polyester cotton and preparation method thereof | |
| CN111691197B (en) | Washable flame-retardant non-woven fabric and preparation method thereof | |
| JP2001508139A (en) | Crosslinking agent for cellulosic fibers | |
| CN104818607B (en) | Method of producing flame retardant textile by electronic radiation technology | |
| Jinping et al. | Graft copolymerization modification of silk fabric with an organophosphorus flame retardant | |
| CN107177979A (en) | One kind is without molten drop flame retardant polyester fiber/fabric and preparation method thereof | |
| CN112442748A (en) | Preparation method and application of melamine phytate flame-retardant modified acrylic fiber | |
| CN105133319B (en) | Preparation method of molten-drop-resisting polyamide fiber or fabric | |
| Li et al. | Improving the fire performance and washing durability of nylon-cotton blend fabrics by the incorporation taurine derivatives | |
| CN105113205A (en) | Flame retardant tidying method for purified cotton or blended cotton textile fabric | |
| Liu et al. | Epoxidized waste cooking oil enhancing the interfacial binding strength for fully bio-based flame retardant wool fabric with good wearability | |
| CN103898744A (en) | Preparation method of halogen-free flame retardant non-melting nylon66 fabric | |
| US9945068B2 (en) | Flame retardant fabrics and methods for manufacturing the same | |
| CN116427173A (en) | Washable flame-retardant anti-dripping polyester cotton 65/35 fabric and preparation method thereof | |
| CN105200765A (en) | Pure cotton or cotton blended fabric and preparation method thereof | |
| CN101831803B (en) | After-finishing flame resistant method for nylon fabric | |
| CN103361006B (en) | A kind of High-penetration acrylate adhesive for waterproof roll tire fabric and preparation method thereof | |
| CN105386294A (en) | Polyester flame-retardant fabric and manufacturing method thereof | |
| US3839081A (en) | Acrylic fiber having a high water absorbency and a wool-like hand and process therefore | |
| CN1159489C (en) | Non-formaldehyde composition for durably shape-retentive finish of cellulose fabrics and its method | |
| JP2007023458A (en) | Flame-retardant blended yarn |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220119 Address after: 310018 928, 2 Avenue, Xiasha Higher Education Park, Jianggan District, Hangzhou, Zhejiang. Patentee after: ZHEJIANG SCI-TECH University Patentee after: INSTITUTE OF QUARTERMASTER ENGINEERING TECHNOLOGY, INSTITUTE OF SYSTEMS ENGINEERING, ACADEMY OF MILITARY SCIENCES Address before: 310018 928 Baiyang Street, Jianggan Economic Development Zone, Hangzhou City, Zhejiang Province Patentee before: ZHEJIANG SCI-TECH University |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170510 |